CN103050745A - Pretreatment method for lead plaster of waste lead-acid accumulators - Google Patents
Pretreatment method for lead plaster of waste lead-acid accumulators Download PDFInfo
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- CN103050745A CN103050745A CN2013100047060A CN201310004706A CN103050745A CN 103050745 A CN103050745 A CN 103050745A CN 2013100047060 A CN2013100047060 A CN 2013100047060A CN 201310004706 A CN201310004706 A CN 201310004706A CN 103050745 A CN103050745 A CN 103050745A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention belongs to the field of utilizing waste lead-acid accumulators to produce secondary lead, and relates to a novel pretreatment method for lead plaster of the waste lead-acid accumulators. The pretreatment method comprises the steps that after the waste lead-acid accumulators are crushed and subjected to preliminary separation, waste lead plaster is obtained; wet sieving or dry sieving is conducted on the waste lead plaster by a 0.85mm-0.106mm sieve; plate grid and plastic fragment products are obtained; table reconcentration is conducted on undersize products; diaphragm paper products and pure lead plaster are obtained; the plate grid and plastic fragment products and the diaphragm paper products can enter a fire smelting system; the pure lead plaster is treated by a citric acid aqueous solution or sodium carbonate or a new acetic acid leaching technology; and lead powder is obtained, and can be used for preparing the lead-acid accumulators directly. The pretreatment method for the lead plaster of the waste lead-acid accumulators is simple in technological equipment, low in investment, low in cost, high in impurity removal rate, clean, highly-efficient and energy-saving.
Description
Technical field
The invention belongs to lead-acid accumulator and produce the reviver field.The present invention relates to a kind of novel waste lead acid battery lead cream preprocess method.
Background technology
Lead acid accumulator dominate always in secondary battery industry, according to statistics, from 2005 to 2010, China's lead acid accumulator aspect the output value in electrokinetic cell field and sale all in occupation of the secondary cell market index more than 50%.Along with the fast development of China's rapid development of economy, particularly automobile, motorcycle, electric bicycle industry, lead acid accumulator output is just with annual 10% speed increase.
The lead acid accumulator output is larger, and the lead acid accumulator of scrapping is more.According to statistics, the generation of China's lead-acid accumulator in 2007 is about 840,000 tons, and other contain about 200,000 tons of scrap lead lead skim, lead ash etc.Expect 2015, lead-acid accumulator year generation will be above more than 2,000,000 tons.
In the face of the lead-acid accumulator of huge quantity like this, if reasonable disposal and utilization in addition not, the pollution that causes will consist of huge threat to environmental protection, the ecological balance and health.Simultaneously, China's lead ore resource is relatively deficient, and main dependence on import remedies the deficiency of lead ore resource.Under this objective condition, more in the urgent need to the regeneration lead-acid accumulator.
Lead-acid accumulator is through falling after the acid, mainly contains plastic casing, grid, diaphragm paper, scrap lead cream and forms, and in all building blocks, the regeneration of scrap lead cream is maximum difficult point, also is the plumbous key that reclaims in the lead-acid accumulator.At present the main method that adopts of recycling lead of abandoned lead acid accumulator has pyrogenic process and wet method, and pyrogenic process is lead plaster to be fallen carry out pyrometallurgical smelting after the processing such as sour and preliminary break process, obtains plumbous product.Wet method mainly contains two kinds: direct electrowinning method and indirect electrodeposition method.The direct electrowinning method directly places electrolysis tank to carry out electrolytic recovery lead lead plaster.Electrodeposition method need be processed through carrying out electrodeposition after further transforming, leaching again indirectly.
Pyrogenic attack waste lead acid battery lead cream pollutes energy consumption height in large and the production process.Although wet method-electrodeposition process can air conservation, energy consumption is large, and technological process is long, equipment investment is large, be not suitable for little factory and office reason.
" the plumbous recovery " (CN 101573461 B) have invented a kind of method of utilizing aqueous citric acid solution to process plumbous discarded object, the method adopts aqueous citric acid solution to leach plumbous discarded object, lead in the scrap lead cream is converted into lead citrate, then at 250~1100 ℃ of lower roasting lead citrates, obtain lead powder.This technology can be eliminated SO
2And lead dust pollution, reduce energy consumption.The maximum characteristics of this technique are that final products are ultra-fine lead powder, can be directly used in the production high-performance lead-acid accumulator, and this recycles the brand-new technology that a green is provided for lead-acid accumulator." a kind of plumbous method that reclaims " (CN 102560122A) discloses a kind of PbSO of comprising
4, PbO
2, PbO and Pb plumbous discarded object and citric acid solution hybrid reaction, produce lead citrate, then lead citrate is converted into the method for lead or lead oxide.The advantage of above-mentioned technique maximum is to have solved SO in the pyrometallurgical smelting process
2The problem of lead dust volatilization under discharging and the high temperature has also solved the high energy consumption problem of lead plaster wet method electrodeposition process.
It is plumbous no matter to adopt which kind of method to reclaim in the lead-acid accumulator, all needs at first lead-acid accumulator to be carried out fragmentation and preliminary sorting.Patent documentation " lead-acid accumulator cracking and sorting machine and method for separating " CN101979165A), patent documentation " lead-acid accumulator cracking and sorting machine " (CN201848422U), " lead-acid accumulator automatic pulverizing separation system and method " (CN102615095A) etc. disclose relevant device and the method for the broken and sorting of lead-acid accumulator.Patent documentation and existing technology that all above-mentioned lead-acid accumulators carry out broken and preliminary sorting all are to reclaim lead pig with traditional method melting alive to match.Tradition pyrometallurgical smelting technique can make the organic impurities that remains in the lead plaster by high temperature, decompose removal such as plastic casing, diaphragm paper, fiber, carbon black etc., remain in the inorganic impurity in the lead plaster, remove by follow-up refinery practice such as inorganic impurity elements such as the iron in grid fragment, the welding battery joint, copper, antimony.Yet when the lead-acid accumulator crushed product was carried out sorting, lead plaster separated not thorough with other component, and plastic casing and grid fragment, diaphragm paper, fiber, carbon black etc. can be sneaked in the lead plaster the plumbous technique that reclaims of wet method is had a strong impact on generation.When plumbous in adopting above-mentioned aqueous citric acid solution and other leaching method recovery scrap lead cream, the final products lead powder is directly used in when preparing new lead acid accumulator, if impurity exceeds standard in the lead powder, will directly affect the performance of the storage battery of producing, therefore, need impurity content in the strict control lead powder.This just need to control from the source, reduces as far as possible impurity and enters lead powder.So, need before leaching, waste lead acid battery lead cream to be carried out preliminary treatment, remove the impurity that is mingled in the scrap lead cream.But there is no at present correlation technique and research.
Shaking table is a kind of widely used gravitational separation equipment, and separation by shaking table is to utilize the reciprocating motion of bed surface and the flushing action of current that material density is separated.The advantage of separation by shaking table is that accuracy is high, once sorts and can obtain high-grade concentrate or discarded tailing, is usually used in sorting tungsten, tin, niobium, tantalum and gold containing ore.
Summary of the invention
The object of the present invention is to provide the preprocess method of lead plaster in a kind of effective lead-acid accumulator, by screening, gravity treatment, remove impurity in the scrap lead cream, improve waste lead acid battery lead cream wet-leaching technique leaching process conversion ratio, guarantee the quality of final products lead powder, solve the technological difficulties of this technique, promote improving and using of this technique.
The preprocess method of lead plaster in a kind of lead-acid accumulator provided by the invention comprises following steps:
After sour through falling, broken, the preliminary sorting of the 1st step lead-acid accumulator, isolate scrap lead cream;
The 2nd step sieved scrap lead cream with 0.85mm~0.106mm sieve;
The 3rd step adopted shaking table that undersize is carried out gravity treatment, obtained diaphragm paper and pure lead plaster, the purer lead plaster that obtains was leached;
The 4th step Separation of Solid and Liquid obtains the citric acid precursor, at 325~375 ℃ of lower roasting lead citrate precursor 1h~3h, obtains lead powder.
Gravity treatment is the difference according to the density of various materials, thus in moving medium suffered gravity, fluid dynamic and other mechanical forces different, thereby realize the process of pressing density separation.Paste density is maximum in the scrap lead cream, and diaphragm paper, fiber, carbon black density are less, and density variation is larger, and the E value is larger, and Gravity separation is easier to.
The present invention adopts table concentration to remove foreign material in the scrap lead cream.Main leaded material is PbSO in the scrap lead cream
4, PbO
2, PbO and Pb, fine size, and sneak into the foreign material such as material shell in the lead plaster and grid fragment, diaphragm paper, fiber, carbon black, on size and density, there is significant difference with lead plaster, utilize this difference, adopt the method for screening, gravity treatment can realize separating of leaded material and foreign material in the scrap lead cream, thereby obtain purer lead plaster.Particularly, the present invention has following advantage and effect:
1. technique is simple, only needs screening, gravity treatment can remove impurity in the waste lead acid battery lead cream;
2. equipment is simple, only needs vibrating screen, shaking table, invests littlely, and production cost is low;
3. dust removal rate is high, can remove the impurity more than 99.0% in the scrap lead cream, has solved the difficult problem of removal of impurities in the waste lead acid battery lead cream wet-leaching treatment technology.
Description of drawings
Fig. 1 is the schematic flow sheet of the preprocess method of lead plaster in the lead-acid accumulator.
Embodiment
The preprocess method of lead plaster comprises following steps in the lead-acid accumulator provided by the invention:
(1) after sour through falling, broken, the preliminary sorting of lead-acid accumulator, isolates scrap lead cream.
(2) with 0.85mm~the 0.106mm sieve sieves scrap lead cream, but wet screening, but also dry screen, oversize is grid fragment, plastic flakes, diaphragm paper of bulk etc., the foreign material of these bulks can enter the pyrometallurgical smelting system.
(3) adopt shaking table that undersize is processed, obtain two kinds of products, the one, diaphragm paper, the one, pure lead plaster, diaphragm paper can enter the pyrometallurgical smelting system, pure lead plaster can adopt citric acid and natrium citricum mixed aqueous solution to leach, and also can adopt two step lixiviation process, and the first step adopts Sodium Carbonate Leaching, second step adopts citric acid to leach (a scheme), perhaps, the first step adopts acetic acid to leach, and second step adopts natrium citricum to leach (b scheme).When adopting citric acid and natrium citricum mixed solution to leach, lead plaster: citric acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: (2.0~2.6): (1.4~2.0): (0.2~0.4), its preferred value is 1: 2.4: 1.8: 0.3, and liquid-solid ratio is about 4: 1~and 8: 1; When adopting a scheme to leach, lead plaster: sodium carbonate: natrium citricum: the mass ratio of hydrogen peroxide is 1: (0.4~0.8): (0.4~0.8): (0.3~0.6), its preferred value is 1: 0.6: 0.7: 0.5, first paragraph leached liquid-solid ratio 8: 1~10: 1, and second segment leached liquid-solid ratio 4: 1~6: 1; When adopting the b scheme to leach, lead plaster: acetic acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: (0.2~0.5): (1.4~1.8): (0.4~0.8), its preferred value is 1: 0.35: 1.6: 0.6, first paragraph leached liquid-solid ratio 4: 1~8: 1, and second segment leached liquid-solid ratio 4: 1~6: 1.On address the aftermentioned liquid-solid ratio and all refer to mass ratio.
(4) after the leaching, Separation of Solid and Liquid obtains the lead citrate precursor, and it at 325~375 ℃ of lower roasting 1h~3h, is obtained lead powder.Lead powder can be directly used in the preparation lead acid accumulator.
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described further.Need to prove at this, understand the present invention for the explanation of these execution modes for helping, but do not consist of limitation of the invention.In addition, below in each execution mode of described the present invention involved technical characterictic just can mutually not make up as long as consist of each other conflict.
Embodiment 1
Lead-acid accumulator is broken, separation obtain scrap lead cream.Get waste lead acid battery lead cream 10.0kg, sieve with the 0.85mm sieve, obtain oversize 2.1kg, undersize 7.9kg.Undersize is carried out gravity treatment with shaking table, obtain diaphragm paper 0.4kg, pure lead plaster 7.5kg.Add 37.5L water, 18kg citric acid, 13.5kg natrium citricum, 2.25kg hydrogen peroxide in the pure lead plaster that obtains, at normal temperatures, leaching 4h filters, and obtains lead citrate.With lead citrate in Muffle furnace in 350 ℃ of lower roasting 1h, obtain lead powder 5.4kg.Lead powder can be directly used in the preparation lead acid accumulator.As calculated, scrap lead cream removal of impurity 99.1%.
Embodiment 2
Get the waste lead acid battery lead cream 5kg of Hubei company, sieve with the 0.25mm sieve, obtain oversize 1.1kg, undersize 3.9kg.Undersize is carried out gravity treatment with shaking table, obtain diaphragm paper 0.2kg, pure lead plaster 3.7kg.In pure lead plaster, add 37L water, 2.22kg sodium carbonate, behind the leaching 1h, add again the 2.59kg citric acid, leach 1h, filter, obtain lead citrate.With lead citrate in Muffle furnace in 375 ℃ of lower roasting 2h, obtain lead powder 2.8kg.Lead powder can be directly used in the preparation lead acid accumulator.As calculated, scrap lead cream removal of impurity 99.2%.
Embodiment 3
Get certain waste lead acid battery lead cream 15kg of company, sieve with the 0.106mm sieve, obtain oversize 2.4kg, undersize 12.6kg.Undersize is carried out gravity treatment with shaking table, obtain diaphragm paper 0.4kg, pure lead plaster 12.2kg.Add 61L water, 4.27kg acetic acid in pure lead plaster, under the normal temperature, leaching 6h adds 19.5kg natrium citricum, 7.32kg hydrogen peroxide again, and at normal temperatures, leaching 4h filters, and obtains lead citrate.With lead citrate in Muffle furnace in 360 ℃ of lower roasting 3h, obtain lead powder 9.1kg.Lead powder can be directly used in the preparation lead acid accumulator.As calculated, scrap lead cream removal of impurity 99.1%.
Embodiment 4-6
Adopt component and technological parameter in the following table, process according to the method that embodiment 1-3 is same, resulting scrap lead cream removal of impurity is more than 99%.
After gathering, the result of embodiment 4-6 sees the following form.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (8)
1. the preprocess method of lead plaster in the lead-acid accumulator comprises following steps:
After sour through falling, broken, the preliminary sorting of the 1st step lead-acid accumulator, isolate scrap lead cream;
The 2nd step sieved scrap lead cream with 0.85mm~0.106mm sieve;
The 3rd step adopted shaking table that undersize is carried out gravity treatment, obtained diaphragm paper and pure lead plaster, the purer lead plaster that obtains was leached;
The 4th step Separation of Solid and Liquid obtains the citric acid precursor, at 325~375 ℃ of lower roasting lead citrate precursor 1h~3h, obtains lead powder.
2. the preprocess method of lead plaster in the lead-acid accumulator according to claim 1, it is characterized in that, in the 3rd step, pure lead plaster adopts citric acid and natrium citricum mixed aqueous solution to leach, lead plaster: citric acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: (2.0~2.6): (1.4~2.0): (0.2~0.4), liquid-solid ratio is about 4: 1~and 8: 1.
3. the preprocess method of lead plaster in the lead-acid accumulator according to claim 2, it is characterized in that lead plaster: citric acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: 2.4: 1.8: 0.3.
4. the preprocess method of lead plaster in the lead-acid accumulator according to claim 1, it is characterized in that, in the 3rd step, pure lead plaster adopts two step lixiviation process, the first step adopts Sodium Carbonate Leaching, and second step adopts citric acid to leach, and lead plaster in the second step: sodium carbonate: natrium citricum: the mass ratio of hydrogen peroxide is 1: (0.4~0.8): (0.4~0.8): (0.3~0.6), first paragraph leached liquid-solid ratio 8: 1~10: 1, and second segment leached liquid-solid ratio 4: 1~6: 1.
5. the preprocess method of lead plaster in the lead-acid accumulator according to claim 4, it is characterized in that lead plaster: sodium carbonate: natrium citricum: the mass ratio of hydrogen peroxide is 1: 0.6: 0.7: 0.5.
6. the preprocess method of lead plaster in the lead-acid accumulator according to claim 1, it is characterized in that, in the 3rd step, pure lead plaster adopts two step lixiviation process, the first step adopts acetic acid to leach, and second step adopts natrium citricum to leach, and lead plaster in the second step: acetic acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: (0.2~0.5): (1.4~1.8): (0.4~0.8), first paragraph leached liquid-solid ratio 4: 1~8: 1, and second segment leached liquid-solid ratio 4: 1~6: 1.
7. the preprocess method of lead plaster in the lead-acid accumulator according to claim 6, it is characterized in that lead plaster: acetic acid: natrium citricum: the mass ratio of hydrogen peroxide is 1: 0.35: 1.6: 0.6.
8. the preprocess method of lead plaster in the lead-acid accumulator according to claim 1 is characterized in that, in the 3rd step, diaphragm paper enters the pyrometallurgical smelting system and processes.
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CN105161788A (en) * | 2015-09-07 | 2015-12-16 | 超威电源有限公司 | Method for removing ultra-fine glass fiber (AGM) partition plate from waste lead paste in lead-acid storage battery |
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CN105161788A (en) * | 2015-09-07 | 2015-12-16 | 超威电源有限公司 | Method for removing ultra-fine glass fiber (AGM) partition plate from waste lead paste in lead-acid storage battery |
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CN105621392A (en) * | 2016-03-24 | 2016-06-01 | 华中科技大学 | Preparation method and application of three-dimensional porous carbon material |
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